The objective of this thesis was to chemically produce Multiferroic Bismuth Iron Oxide (BiFeO3) (BFO) and cobalt doped Bismuth Iron Oxide (BFCO) nanoparticles for photovoltaic applications. The syntheses in these materials were made using the sol-gel method. To determine the crystallite size from XRD, understand the light response of these materials, the UV-Vis absorption and the vibrational energy levels of the bonds by FTIR were made. During the process of the chemical synthesis, the annealing temperature was set at 450℃ for 2 h. From the XRD measurement, the observation of the peaks and the average crystallite size of BFO and BFCO were 20 nm and 22 nm respectively. It indicates no secondary phase was obtained in the diffraction patterns suggested single phase formation of Cobalt doped Bismuth ferrite nanoparticles. The optical band gap energy measurements on BFO and BFCO were at 2.43 eV and 2.326 eV respectively. Further, the FTIR vibrational emission spectrum showed that the O-H single bond on 3417 cm -1 the BFO and BFCO in the range 1000–4000 cm-1 . The prominent vibration was observed at 3417, 1390, 970, and 556 cm-1 . The sharp peak in the band range 400_ 1000 cm-1 is attributed to metal–oxygen / Fe-O, Bi-O stretching vibration, and O-Fe-O bending vibration in BFO and BFCO.